US3364152A - Process for the manufacture of a boron, aluminum or alkaline earth metal, and carbon composition and product - Google Patents

Process for the manufacture of a boron, aluminum or alkaline earth metal, and carbon composition and product Download PDF

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Publication number
US3364152A
US3364152A US362487A US36248764A US3364152A US 3364152 A US3364152 A US 3364152A US 362487 A US362487 A US 362487A US 36248764 A US36248764 A US 36248764A US 3364152 A US3364152 A US 3364152A
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Prior art keywords
boron
aluminum
alkaline earth
carbon
reaction
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Expired - Lifetime
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US362487A
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English (en)
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Lipp Alfred
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Elektroschmelzwerk Kempten GmbH
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Elektroschmelzwerk Kempten GmbH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C7/00—Control of nuclear reaction
    • G21C7/06—Control of nuclear reaction by application of neutron-absorbing material, i.e. material with absorption cross-section very much in excess of reflection cross-section
    • G21C7/24—Selection of substances for use as neutron-absorbing material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Definitions

  • Extremely hard products comprising boron, carbon and aluminum have previously been produced.
  • Such compositions contained 2-5% of aluminum in the free, or at least not bound to oxygen form, the remainder of the composition constituting the boron and the carbon in the form of boron carbide varying in composition between B C and B C.
  • Such compositions were produced by heating boron carbide of B C-B C composition with an excess of aluminum in a graphite mold at a pressure of at least 35 kg./cm. at a temperature ranging from 1800 to 1900 C., Al C being formed if a temperature below 1800 C. was used.
  • the composition produced by this method under pressure and heat must be ground to the desired grain size, with great difliculty because of its extreme hardness.
  • Borides of the alkaline earth metals have also previously been produced by reacting mixtures of a finely divided alkaline earth metal and finely divided boron in a protective gas atmosphere.
  • Magnesium tetraboride could be produced in this manner by heating a mixture of finely divided boron and magnesium either in the presence of an inert atmosphere or in vacuo to a temperature ranging from 900 to 1200 0., followed by treating the resulting reaction mixture with dilute acids to remove everything except the magnesium tetraboride.
  • amorphous boron and beryllium oxide are reacted with each other in an electric furnace, whereby a hard, crystalline, insoluble crystalline residue is obtained.
  • the reactions above described will be greatly facilitated if the boron carbide has a very great surface, i.e. if very fine grains thereof are employed.
  • the fineness of the grinding is of lesser importance. Any known method can be used for obtaining the boron carbide in the desired degree of fineness.
  • the ratio of boron to carbon appears to be of little importance.
  • use may be made of boron carbide high in carbon, such as B 0 for which there are few industrial uses.
  • use may be made of carbides high in boron, such as B C.
  • the procedures of the present invention permit the production of final products, which after completion of the reaction and the treatment of the residue with acids or other conventional method for the separation of the undesired by-products, are remarkably constant in composition.
  • the reaction is preferably carried out in an inert atmosphere.
  • a stream of hydrogen or argon can be conveniently used.
  • gases inert under the conditions of the reaction may, however, be used. It is important, however, that the gas used does not contain any carbon compound such as carbon monoxide.
  • a preferred composition of the type contemplated by this invention is one which contains boron, aluminum and carbon in which chemically bound aluminum is present to the extent of about 720%, and chemically bound carbon to the extent of about 12-16%, the remainder being boron.
  • stoichiometric amounts of the boron carbide and alkaline earth metal are preferably used, although it is possible to use an excess of either type of reactant so as to affect the properties of the final product in any desired manner.
  • a particular advantage of the procedure of the present invention consists in rendering it possible to obtain an alkaline earth boride which is substantially free from carbon, the alkaline earth carbide formed in the process being separated from the reaction mixture in accordance with known procedures.
  • the reaction product is first treated with water, some hydrolysis products remaining which can then be completely removed by acid treatment. Or, the reaction product may simply be subjected to acid treatment.
  • An especial advantage of the process of the present invention lies in the fact that it permits the substantially complete reaction of the boron and carbon present in the starting materials and the production of products of technical importance.
  • B 0 is used as the source of boron
  • metal oxides are produced in the reaction and can only be separated from the reaction products with the greatest of difiiculty. It is well known that the preparation of pure alkaline earth borides could ,only be accomplished with the greatest of difiiculty by prior processes, as compared to the relative simplicity and ease by the process of the present invention.
  • Still another advantage of the process of the present invention lies in the fact that it requires substantially smaller quantities of the valuable starting materials than in the case of the processes of the prior art.
  • CaB only /6 as much would be required for the production of the desired product.
  • the process of the present invention will be illustrated by the following specific examples. It is understood, however, that variations from the procedures of these specific examples can be employed Without departing from the concept of the invention disclosed and claimed here-
  • the hard products rich in boron produced by the process of the present invention can also be used as grinding agents in loose or bonded form besides their use as fireproof materials. Because of the high temperature and oxidation resistance they are preferred as fireproof materials, while the high boron content enables their use as neutron absorber in the field of atomic energy.
  • EXAMPLE I A dry shaped article pressed from a mixture of powdered boron carbide and powdered aluminum was placed in a combustion boat in a silite tube furnace provided with a ceramic protective tube. The article was then subjected to the temperatures shown in Table 1 below, using either hydrogen or argon as the inert gas. Instead of using a dry article one containing a volatile binder, such as trichlorethylene gave similar results.
  • the boron carbide used in each experiment had a boron content of 78.2% and a carbon content of 21.8%.
  • Table II The starting material, as shown in line 1 of Table I, was composed of 75.5% boron, 10.0% aluminum and 4 EXAMPLE n An intimate mixture of 50 parts by weight of boron carbide and 50 parts by weight of beryllium metal was prepared and the resulting mixture reacted in a high melting crucible at a temperature of 1300 in an atmosphere of hydrogen. In order to obtain pure beryllium boride the resulting reaction mixture was treated with dilute acetic acid. There was thus obtained a product having a boron assay of 69.7% and a beryllium assay of 30.1%. The density of the beryllium boride was 2.31 g./ccm., and its Knoop hardness was 3200 kg./mrn. under a load of g. The reaction apparently took place in accordance with the following equation:
  • EXAMPLE III An intimate mixture of 65 parts by weight of finely divided magnesium metal and 35 parts by weight of finely divided boron carbide was heated in a combustion boat of sintered carborundum for four hours at 750 C. in an atmosphere of hydrogen. The resulting reaction product dissolved completely in dilute, hot mineral acids (hydrochloric or sulfuric). As an indication of this it might be noted that during the acid treatment the typical odor of boron hydride was observed.
  • the evaporation of the magnesium is lowered by raising the pressure at which the reaction takes place and accordingly the reaction equilibrium is shifted and the yields are improved.
  • Process for the manufacture of boride-containing compositions which comprises reacting at elevated temperatures boron carbide with a material selected from the group consisting of finely divided aluminum metal and finely divided alkaline earth metals, and recovering the boride-containing compositions from the reaction products.
  • Process for the manufacture of boride-containing compositions which comprises heating in an inert atmosphere to temperatures ranging from 600 to 1500 C. a mixture of finely divided boron carbide and a finely divided material selected from the group consisting of aluminum metal and alkaline earth metals, the reaction temperature ranging from 1000 to 1500 C. in the case of aluminum metal, and from 600 to 1500 C. in the case of the alkaline earth metals, and recovering from the reaction products boride-containing compositions.
  • boron carbide has the composition of 78.2%, by weight, boron and 21.2%, by weight, carbon.
  • compositions suitable for use as neutron absorbers consisting of boron, aluminum and carbon, with the overall composition B C Al, having a boron carbide structure and showing a region of homogeneity of 720%, by

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Ceramic Products (AREA)
  • Carbon And Carbon Compounds (AREA)
US362487A 1964-01-23 1964-04-24 Process for the manufacture of a boron, aluminum or alkaline earth metal, and carbon composition and product Expired - Lifetime US3364152A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEE26282A DE1229505B (de) 1964-01-23 1964-01-23 Verfahren zur Herstellung von Erdalkalimetallboriden und -carbiden

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AT (1) AT263698B (de)
DE (1) DE1229505B (de)
GB (1) GB1070325A (de)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4104062A (en) * 1969-08-13 1978-08-01 Norton Company Process for making aluminum modified boron carbide and products resulting therefrom
USRE30193E (en) * 1973-05-23 1980-01-15 Fire retardant agent
JPS6212673A (ja) * 1985-05-06 1987-01-21 ザ　リ−ジエンツ　オブ　ザ　ユニバ−シテイ　オブ　カリフオルニア ほう素−炭化物−アルミニウム及びほう素−炭化物−反応性金属サ−メツト
US4702770A (en) * 1985-07-26 1987-10-27 Washington Research Foundation Multipurpose boron carbide-aluminum composite and its manufacture via the control of the microstructure
US4894286A (en) * 1988-11-07 1990-01-16 Rohr Industries, Inc. Oxidation resistant refractory coated carbon-carbon composites
EP0322336A3 (en) * 1987-12-23 1990-07-11 Lanxide Technology Company,Lp Process for preparing selfsupporting bodies and products made thereby
EP0378501A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zum Verbinden eines keramischen Verbundwerkstoffkörpers mit einem zweiten Körper und so hergestellte Gegenstände
EP0378504A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zur Herstellung von selbsttragenden Körpern mit kontrollierter Porosität und abgestuften Eigenschaften sowie damit hergestellte Körper
EP0378503A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zur Modifizierung eines keramischen Verbundwerkstoffkörpers durch eine Nachbehandlung und so hergestellte Gegenstände
EP0322341A3 (en) * 1987-12-23 1990-08-01 Lanxide Technology Company,Lp A method of producing and modifying the properties of ceramic composite bodies
EP0383715A1 (de) * 1989-01-13 1990-08-22 Lanxide Technology Company, Lp. Verfahren zum Herstellen keramischer Verbundwerkstoffkörper
US20030042647A1 (en) * 2001-08-29 2003-03-06 Pyzik Aleksander J. Boron containing ceramic-aluminum metal composite and method to form the composite

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2461821C3 (de) * 1974-12-30 1984-10-18 Elektroschmelzwerk Kempten GmbH, 8000 München Verfahren zur Herstellung von hexagonalem Bornitrid

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2746133A (en) * 1951-10-16 1956-05-22 Norton Co Process of making boron carbide containing aluminum, and products thereof
GB878465A (en) * 1959-12-28 1961-09-27 Ici Ltd Neutron-absorbing material
GB884577A (en) * 1957-09-06 1961-12-13 Commissariat Energie Atomique Improvements in methods of preparing sintered beryllium oxide products
US3108886A (en) * 1958-12-29 1963-10-29 Carborundum Co Hard, refractory crystalline materials
US3153636A (en) * 1958-10-31 1964-10-20 Carborundum Co Porous bodies of controlled densities and methods of making them
US3178807A (en) * 1961-10-05 1965-04-20 Du Pont Cermet of aluminum with boron carbide or silicon carbide

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2746133A (en) * 1951-10-16 1956-05-22 Norton Co Process of making boron carbide containing aluminum, and products thereof
GB884577A (en) * 1957-09-06 1961-12-13 Commissariat Energie Atomique Improvements in methods of preparing sintered beryllium oxide products
US3153636A (en) * 1958-10-31 1964-10-20 Carborundum Co Porous bodies of controlled densities and methods of making them
US3108886A (en) * 1958-12-29 1963-10-29 Carborundum Co Hard, refractory crystalline materials
GB878465A (en) * 1959-12-28 1961-09-27 Ici Ltd Neutron-absorbing material
US3178807A (en) * 1961-10-05 1965-04-20 Du Pont Cermet of aluminum with boron carbide or silicon carbide

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4104062A (en) * 1969-08-13 1978-08-01 Norton Company Process for making aluminum modified boron carbide and products resulting therefrom
USRE30193E (en) * 1973-05-23 1980-01-15 Fire retardant agent
JPS6212673A (ja) * 1985-05-06 1987-01-21 ザ　リ−ジエンツ　オブ　ザ　ユニバ−シテイ　オブ　カリフオルニア ほう素−炭化物−アルミニウム及びほう素−炭化物−反応性金属サ−メツト
JPH0776128B2 (ja) 1985-05-06 1995-08-16 ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア 炭化ほう素―アルミニウム及び炭化ほう素―反応性金属サーメット
US4702770A (en) * 1985-07-26 1987-10-27 Washington Research Foundation Multipurpose boron carbide-aluminum composite and its manufacture via the control of the microstructure
WO1987000557A3 (en) * 1985-07-26 1988-09-07 Washington Res Found A multipurpose boron carbide-aluminum composite and its manufacture via the control of the microstructure
EP0322341A3 (en) * 1987-12-23 1990-08-01 Lanxide Technology Company,Lp A method of producing and modifying the properties of ceramic composite bodies
EP0322336A3 (en) * 1987-12-23 1990-07-11 Lanxide Technology Company,Lp Process for preparing selfsupporting bodies and products made thereby
US4894286A (en) * 1988-11-07 1990-01-16 Rohr Industries, Inc. Oxidation resistant refractory coated carbon-carbon composites
EP0378504A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zur Herstellung von selbsttragenden Körpern mit kontrollierter Porosität und abgestuften Eigenschaften sowie damit hergestellte Körper
EP0378503A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zur Modifizierung eines keramischen Verbundwerkstoffkörpers durch eine Nachbehandlung und so hergestellte Gegenstände
EP0383715A1 (de) * 1989-01-13 1990-08-22 Lanxide Technology Company, Lp. Verfahren zum Herstellen keramischer Verbundwerkstoffkörper
AU628461B2 (en) * 1989-01-13 1992-09-17 Lanxide Corporation A process for preparing self-supporting bodies having controlled porosity and graded properties and products produced therby
US5299621A (en) * 1989-01-13 1994-04-05 Lanxide Technology Company, Lp Method of producing ceramic composite bodies
EP0378501A1 (de) * 1989-01-13 1990-07-18 Lanxide Technology Company, Lp. Verfahren zum Verbinden eines keramischen Verbundwerkstoffkörpers mit einem zweiten Körper und so hergestellte Gegenstände
US20030042647A1 (en) * 2001-08-29 2003-03-06 Pyzik Aleksander J. Boron containing ceramic-aluminum metal composite and method to form the composite
US6835349B2 (en) 2001-08-29 2004-12-28 The Dow Chemical Company Boron containing ceramic-aluminum metal composite and method to form the composite
US20050081963A1 (en) * 2001-08-29 2005-04-21 Pyzik Aleksander J. Boron containing ceramic-aluminum metal composite and method to form the composite
US7160627B2 (en) 2001-08-29 2007-01-09 The Dow Chemical Company Boron containing ceramic-aluminum metal composite and method to form the composite

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DE1229505B (de) 1966-12-01
GB1070325A (en) 1967-06-01
AT263698B (de) 1968-07-25

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